JP3828821B2 - Liquid material vaporizer - Google Patents

Liquid material vaporizer Download PDF

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JP3828821B2
JP3828821B2 JP2002069131A JP2002069131A JP3828821B2 JP 3828821 B2 JP3828821 B2 JP 3828821B2 JP 2002069131 A JP2002069131 A JP 2002069131A JP 2002069131 A JP2002069131 A JP 2002069131A JP 3828821 B2 JP3828821 B2 JP 3828821B2
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liquid material
gas
gas flow
liquid
temperature
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JP2003273026A (en
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英顕 宮本
均 北川
哲夫 清水
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Horiba Stec Co Ltd
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Horiba Stec Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/52—Controlling or regulating the coating process
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
    • C23C16/4482—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material by bubbling of carrier gas through liquid source material

Description

【０００１】
【発明の属する技術分野】
この発明は、例えば半導体製造において用いられる各種のガスを、液体材料を気化することによって供給するための液体材料気化供給装置に関する。
【０００２】
【従来の技術】
従来の液体材料気化供給装置として、恒温槽内に液体材料を加熱し気化させるためのするための材料タンクと、この材料タンクにおいて生じたガスの流量を制御するマスフローコントローラとを設けたものがある。図３はこのような液体材料気化供給装置を概略的に示すもので、この図において、３１は適宜の温度に設定された恒温槽で、その内部には、液体材料ＬＭを収容し、この液体材料ＬＭを加熱するためのヒータ３２を備えた材料タンク３３が設けられている。この材料タンク３３には、液体材料ＬＭを供給する液体材料供給管３４と、材料タンク３３において発生したガスを導出するガス導出管３５が接続されている。そして、液体材料供給管３４には開閉弁３６が設けられ、ガス導出管３５の恒温槽３１内の部分には高温用マスフローコントローラ３７が設けられている。
【０００３】
上記構成の液体材料気化供給装置においては、液体材料ＬＭを収容した材料タンク３３がヒータ３２によって加熱されると、その内部の温度が上昇し、液体材料ＬＭの蒸気圧が高められ、これによって液体材料ＬＭが気化されて所定のガスになる。この発生ガスは、材料タンク３３とガス導出管３５との圧力差を得ることで、高温用マスフローコントローラ３７で直接流量制御して外部に取り出され、図示していないユースポイント（例えば半導体製造装置）方向に送られる。
【０００４】
【発明が解決しようとする課題】
ところで、前記図３に示した液体材料気化供給装置においては、材料タンク３３内の液体材料ＬＭの液量は、図示していないが、フロートを利用した液面計によって検出され、前記液体材料ＬＭが所定の量以下になったときには、液体材料供給管３４に設けられた開閉弁３６を開いて材料タンク３３内に液体材料ＬＭが供給される。この場合、供給される液体材料ＬＭによって材料タンク３３内の液体材料ＬＭの温度が低下し、所望のガス発生が行われにくくなるところから、前記液体材料ＬＭの供給の都度、ガス発生が中断されることになり、したがって、気化ガスの連続発生および連続供給を行うことができないといった不都合があった。
【０００５】
また、高温用マスフローコントローラ３７でガスの流量制御を行う場合、制御弁部での断熱膨張による熱を供給する必要があるところから、高温用マスフローコントローラ３７の温度を材料タンク３３における温度よりも１０℃程度高く設定する必要があった。このため、高温用マスフローコントローラ３７に組み込まれている流量センサ部の温度がこれに伴って高くならざるを得ず、その結果、高温用マスフローコントローラ３７による発生ガスの流量制御の安定性および信頼性の低下を来すといった不都合があった。
【０００６】
さらに、上記従来の液体材料気化供給装置においては、恒温槽３１内に材料タンク３３や高温用マスフローコントローラ３７を収容していたため、装置全体が大型にならざるを得ないといった構成上の不都合もあった。
【０００７】
この発明は、上述の事柄に留意してなされたもので、その目的は、連続的に気化ガスを発生させることができるとともに、発生した気化ガスを精度よく安定して流量制御することができる、信頼性の高い小型コンパクトな液体材料気化供給装置を提供することである。
【０００８】
【課題を解決するための手段】
上記目的を達成するため、請求項１に記載の発明では、液体材料を収容し、この液体材料を加熱して所定のガスを発生させる材料タンクと、この材料タンクに液体材料を供給するための液体材料供給管と、前記材料タンクにおいて発生したガスを導出するガス導出管を備えてなる液体材料気化供給装置において、前記材料タンクにこれを専用的に加熱する加熱装置を設けるとともに、前記ガス導出管にガス流量計およびガス流量制御弁を互いに独立した状態で設け、前記ガス流量計およびガス流量制御弁を個別に温度制御するように構成され、さらに、前記ガス流量制御弁は、前記材料タンクの設定温度よりも高い温度に加熱保温されるよう温度制御されており、また、前記ガス流量計は、前記材料タンクの設定温度よりも高く、かつ、前記ガス流量制御弁よりも低い温度に加熱保温されるよう温度制御されている。
【０００９】
上記請求項１に記載の発明によれば、ガス流量制御弁については、断熱膨張による熱を補うため、材料タンクよりも例えば１０℃程度高い温度に設定することができる。この場合、ガス流量計は、前記ガス流量制御弁より５〜８℃程度低い温度に設定することができる。したがって、気化ガスを精度よく測定しこれを精度よく流量制御することができる。そして、材料タンクに専用の加熱装置を設けているので、大きな恒温槽が不要になる。
【００１０】
そして、請求項２に記載の発明では、液体材料を収容し、この液体材料を加熱して所定のガスを発生させる材料タンクと、この材料タンクに液体材料を供給するための液体材料供給管と、前記材料タンクにおいて発生したガスを導出するガス導出管を備えてなる液体材料気化供給装置において、前記材料タンクにこれを専用的に加熱する加熱装置を設けるとともに、前記液体材料供給管に、前記材料タンクに供給される液体材料を予熱するための予熱装置および材料タンクに供給される液体材料の流量調整を行うための液体流量調整装置を設け、また、前記ガス導出管にガス流量計およびガス流量制御弁を互いに独立した状態で設け、前記ガス流量計およびガス流量制御弁を個別に温度制御するように構成され、さらに、前記ガス流量制御弁は、前記材料タンクの設定温度よりも高い温度に加熱保温されるよう温度制御されており、また、前記ガス流量計は、前記材料タンクの設定温度よりも高く、かつ、前記ガス流量制御弁よりも低い温度に加熱保温されるよう温度制御されている。
【００１１】
上記請求項２に記載の発明によれば、上記請求項１に記載の発明の効果に加えて、以下の効果を得ることができる。すなわち、上記請求項２に記載の発明によれば、材料タンクに供給される液体材料がその供給前に予熱されるとともに、その供給量が制限されるので、材料タンク内における気化に悪影響が及ぼされることがなく、気化ガス発生中においても液体材料の供給を行うことができる。
【００１２】
【００１３】
【００１４】
【発明の実施の形態】
以下、この発明の詳細を、図を参照しながら説明する。図１は、この発明の液体材料気化供給装置の構成の一例を概略的に示すもので、この図において、１は材料タンクで、液体材料ＬＭを収容するとともに、例えばその上面を除く周囲全体に加熱装置としてのヒータ２が設けられて専用的に加熱保温され、内部に収容された液体材料ＬＭを所定の温度で加熱して気化ガスＧを発生させるように構成されている。なお、図示は省略しているが、材料タンク１には、適宜の液面検出センサが設けられており、液体材料ＬＭの液面が所定の液面レベルまで低下するとこれを検出し、材料補給信号を出力するように構成されている。
【００１５】
３は材料タンク１に液体材料ＬＭを供給するための液体材料供給管で、材料タンク１に供給される液体材料ＬＭを予熱するための予熱装置４と前記液体材料ＬＭの流量調整を行うための液体流量調整装置５が例えばこの順で直列に設けられており、予熱装置４の上流側の液体材料供給管３は、適宜の配管を介して液体材料ＬＭを収容した液体材料供給源（図示していない）に接続されている。そして、予熱装置４は、例えばヒータよりなり、これが液体材料供給管３の外周に巻設されている。また、液体流量調整装置５は、例えば液体用マスフローコントローラよりなり、ヒータなどの加熱装置６によって所定の温度に加熱保温されるように構成されている。
【００１６】
７は材料タンク１内において発生した気化ガスＧを導出するガス導出管で、ガス流量計８、ガス流量制御弁９および開閉弁１０が例えばこの順で互いに独立した状態で設けられており、開閉弁１０の下流側のガス導出管７は、適宜の配管を介してユースポイント（図示していない）に接続されている。そして、ガス流量計８は、例えばガス用マスフローメータよりなり、ヒータなどの加熱装置１１によって所定の温度に加熱保温されるように構成されている。また、ガス流量制御弁９は、例えばピエゾアクチュエータ９ａによってバルブの開度が制御されるピエゾバルブなどガス用制御バルブよりなり、ヒータなどの加熱装置１２によって所定の温度に加熱保温されるように構成されている。
【００１７】
そして、１３は材料タンク１の加熱装置２、液体材料供給管３に設けられる液体材料ＬＭの予熱装置４、液体流量調整装置５の加熱装置６、ガス流量計８の加熱装置１１およびガス流量制御弁９の加熱装置１２を、それぞれ、個別に温度制御する温度コントローラで、液体材料気化供給装置全体を制御する制御装置としてのパソコン１４からの指令に基づいて、前記各加熱装置２，４，６，１１，１２を温度制御する。そして、パソコン１４は、液体流量調整装置５およびガス流量計８からの検出出力が入力され、これに基づいて所定の演算を行って液体流量やガス流量を求めたり、また、これらの演算結果に基づいて液体流量調整装置５およびガス流量制御弁９に所定の制御信号を出力する機能や、材料タンク１に設けられた液面検出センサからの検出信号に基づいて液体流量調整装置５に所定の開度信号を出力する機能などを備えている。
【００１８】
次に、上記構成の液体材料気化供給装置の動作について説明すると、材料タンク１内の液体材料ＬＭを加熱して気化ガスＧを発生させるに際して、所望のガスＧを連続的かつ安定に発生させるために、液体材料ＬＭの種類に応じた最適の状態で気化が行われるように、材料タンク１の加熱温度Ｔ℃を設定する。このとき、液体材料供給管３に設けられる予熱装置４の温度は、これによって予熱される液体材料ＬＭが材料タンク１内に供給しても、材料タンク１内における液体材料ＬＭの気化を妨げない程度のに設定される。そして、液体材料供給管３に設けられる液体流量調整装置としての液体用マスフローコントローラ５は、加熱装置６によって前記液体材料ＬＭの温度を低下させない程度の温度に加熱保温される。一方、ガス導出管７に設けられるガス流量制御弁としてのガス用ピエゾバルブ９の温度は、断熱膨張による熱を補うため、材料タンク１の設定温度Ｔ℃よりも１０℃程度高い温度に加熱保温される。そして、ガス導出管７に設けられるガス流量計８としてガス用マスフローメータは、ガス流量制御弁９の設定温度より５〜８℃程度低い温度になるように加熱保温される。
【００１９】
上記の液体材料気化供給装置においては、通常、液体流量調整装置５は閉じられている。この状態で、液体材料ＬＭを収容した材料タンク１を加熱装置２によって加熱することにより、その内部の温度が上昇し、液体材料ＬＭの蒸気圧が高められ、これによって液体材料ＬＭが気化されて所定の気化ガスＧが発生する。この気化ガスＧは、材料タンク１とガス導出管７との圧力差を得ることで、ガス導出管７に導出される。このガス導出管７には、ガス流量計８およびガス流量制御弁９が互いに独立した状態で設けられているが、ガス流量制御弁９は、材料タンク１の設定温度Ｔ℃よりも１０℃程度高い温度に加熱保温されているので、断熱膨張による熱を十分補うことができ、前記気化ガスＧを精度よく流量調整することができる。また、ガス流量計８は、ガス流量制御弁９よりも５〜８℃程度低い温度に加熱保温されているので、前記気化ガスＧの流量を精度よく測定することができ、したがって、ガス導出管７に導出された気化ガスＧは、開閉弁１０を経て、ユースポイント方向に所定の流量で流れていく。
【００２０】
そして、前記材料タンク１内の液体材料ＬＭがある一定量以下になると、液面検出センサから所定の信号がパソコン１４に送られる。この信号入力により、パソコン１４から所定の信号が予熱装置４および加熱装置６に送られて、これらが所望の加熱動作に入る。そして、所定の時間経過後、液体流量調整装置５が開くことにより、新しい液体材料ＬＭが材料タンク１に補給される。この場合、補給される液体材料ＬＭは、予熱装置４によって所定の温度に加熱（予熱）されるとともに、その供給される量が液体流量調整装置５によって制限（調整）されるので、この液体材料ＬＭの補給によって、材料タンク１内の液体材料ＬＭの気化が妨げられることはない。つまり、液体材料ＬＭの補給中においても材料タンク１内の液体材料ＬＭは温度が低下したりせず、加熱によって気化し、気化ガスＧの発生を維持する。
【００２１】
上述のように、上記構成の液体材料気化供給装置においては、液体材料供給管３に、材料タンク１に供給される液体材料ＬＭ予熱するための予熱装置４および前記液体材料ＬＭの流量調整を行うための液体流量調整装置５を設けているので、材料タンク１内の液体材料ＬＭが少なくなったときに補充のために供給される液体材料ＬＭがその供給前に予熱されるとともに、その供給量が所望の流量となるように制限されるので、材料タンク１内における気化に悪影響が及ぼされることがなく、気化ガス発生中においても液体材料ＬＭの供給を行うことができる。そして、気化ガスＧを導出するガス導出管７に設けられるガス流量計８およびガス流量制御弁９をそれぞれの機能が最も発揮されるように、それぞれ独立して温度制御されるので、気化ガスＧを精度よく測定しこれを精度よく流量制御することができる。さらに、材料タンク１を専用の加熱装置２によって加熱するようにしているので、液体材料ＬＭの気化を最良の条件で行わせるための温度になるように自在に温度調整することができる。
【００２２】
さらに、材料タンク１に加熱装置２を設け、液体材料供給管３に予熱装置４を設け、液体流量調整装置５に加熱装置６を設け、ガス流量計８に加熱装置１１を設け、ガス流量制御弁９に加熱装置１２を設けるとともに、これらをそれぞれ最適の温度になるように加熱保温しているので、図３に示したような恒温槽３１を設ける必要がなく、全体として小型コンパクトな液体材料気化供給装置を構成することができる。
【００２３】
この発明は、上述の実施の形態に限られるものではなく、例えば、図２に示すように、ガス流量制御弁９として、シャットオフ可能な空圧弁９Ｂを一体的に設けたものを用いてもよい。
【００２４】
そして、上記図１および図２のいずれの液体材料気化供給装置においても、ガス流量計８として高温用マスフローメータを用い、かつそのセンサ部として太径のキャピラリを使用した場合、センサ部における圧損を低減することができ、より小型化が促進され、しかも、低温度化によってより信頼度を高めることができる。
【００２５】
なお、液体流量調整装置５としては、制限オリフィスを用いることもできる。
【００２６】
また、液体材料供給管３における予熱装置４と液体流量調整装置５の配置関係を図示例のものと逆にしてもよく、さらに、ガス導出管７におけるガス流量計８とガス流量制御弁９の配置関係を図示例のものと逆にしてもよい。
【００２７】
【発明の効果】
以上のように、この発明の液体材料気化供給装置によれば、材料タンクに対して液体材料を供給するときにおいても、材料タンク内における液体材料の気化が中断されることがない。したがって、液体材料を連続的かつ安定に気化させて所望の気化ガスを発生させることができるとともに、発生した気化ガスを精度よく安定して流量制御することができる。そして、従来のように、材料タンクを恒温槽に収容する必要がないので、装置全体を小型コンパクトに構成することができる。つまり、この発明によれば、小型で信頼性の高い液体材料気化供給装置が得られる。
【図面の簡単な説明】
【図１】 この発明の液体材料気化供給装置の構成の一例を概略的に示す図である。
【図２】 前記液体材料気化供給装置の構成の他の例を概略的に示す図である。
【図３】 従来技術を説明するための図である。
【符号の説明】
１…材料タンク、２…加熱装置、３…液体材料供給管、４…予熱装置、５…液体流量調整装置、７…ガス導出管、８…ガス流量計、９…ガス流量制御弁、ＬＭ…液体材料、Ｇ…気化ガス。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a liquid material vaporization supply device for supplying various gases used in, for example, semiconductor manufacturing by vaporizing a liquid material.
[0002]
[Prior art]
As a conventional liquid material vaporization and supply apparatus, there is one provided with a material tank for heating and vaporizing a liquid material in a thermostat and a mass flow controller for controlling the flow rate of gas generated in the material tank. . FIG. 3 schematically shows such a liquid material vaporizing and supplying apparatus. In this figure, reference numeral 31 denotes a thermostatic bath set to an appropriate temperature, in which the liquid material LM is accommodated and this liquid is stored. A material tank 33 provided with a heater 32 for heating the material LM is provided. The material tank 33 is connected to a liquid material supply pipe 34 that supplies the liquid material LM and a gas outlet pipe 35 that leads out gas generated in the material tank 33. The liquid material supply pipe 34 is provided with an open / close valve 36, and a high temperature mass flow controller 37 is provided in a portion of the gas outlet pipe 35 in the thermostatic chamber 31.
[0003]
In the liquid material vaporizing and supplying apparatus having the above-described configuration, when the material tank 33 containing the liquid material LM is heated by the heater 32, the temperature inside the tank rises, and the vapor pressure of the liquid material LM is increased. The material LM is vaporized into a predetermined gas. The generated gas obtains a pressure difference between the material tank 33 and the gas outlet pipe 35, and is directly controlled by the high-temperature mass flow controller 37 to be taken out to the outside. A use point (not shown) (for example, a semiconductor manufacturing apparatus) Sent in the direction.
[0004]
[Problems to be solved by the invention]
By the way, in the liquid material vaporizing and supplying apparatus shown in FIG. 3, the liquid amount of the liquid material LM in the material tank 33 is not shown, but is detected by a liquid level gauge using a float, and the liquid material LM Is less than a predetermined amount, the on-off valve 36 provided in the liquid material supply pipe 34 is opened, and the liquid material LM is supplied into the material tank 33. In this case, since the temperature of the liquid material LM in the material tank 33 is lowered by the supplied liquid material LM and it becomes difficult to generate a desired gas, the gas generation is interrupted each time the liquid material LM is supplied. Therefore, there is a disadvantage that continuous generation and continuous supply of vaporized gas cannot be performed.
[0005]
Further, when the gas flow rate control is performed by the high-temperature mass flow controller 37, it is necessary to supply heat due to adiabatic expansion at the control valve unit. It was necessary to set it as high as about ° C. For this reason, the temperature of the flow rate sensor unit incorporated in the high-temperature mass flow controller 37 inevitably increases, and as a result, the stability and reliability of the flow control of the generated gas by the high-temperature mass flow controller 37. There was an inconvenience such as lowering.
[0006]
Further, in the conventional liquid material vaporizing and supplying apparatus, since the material tank 33 and the high-temperature mass flow controller 37 are accommodated in the thermostatic chamber 31, there is a structural inconvenience that the entire apparatus must be large. It was.
[0007]
The present invention has been made in consideration of the above-mentioned matters, and its purpose is to continuously generate vaporized gas and to control the flow rate of the generated vaporized gas with high accuracy and stability. It is an object of the present invention to provide a highly reliable and compact liquid material vaporizing and supplying apparatus.
[0008]
[Means for Solving the Problems]
In order to achieve the above object, according to the first aspect of the present invention, there is provided a material tank for storing a liquid material, heating the liquid material to generate a predetermined gas, and supplying the liquid material to the material tank. In the liquid material vaporization supply device comprising a liquid material supply pipe and a gas lead-out pipe for leading out the gas generated in the material tank, the material tank is provided with a heating device dedicated to heating the material tank, and the gas lead-out The pipe is provided with a gas flow meter and a gas flow control valve independently from each other, and is configured to individually control the temperature of the gas flow meter and the gas flow control valve, and the gas flow control valve further includes the material tank. The temperature is controlled so as to be heated and maintained at a temperature higher than the set temperature, and the gas flow meter is higher than the set temperature of the material tank, and Is temperature controlled so as to be heated maintained at a temperature lower than the scan rate control valve.
[0009]
According to the first aspect of the present invention, the gas flow rate control valve can be set to a temperature that is, for example, about 10 ° C. higher than the material tank in order to compensate for heat generated by adiabatic expansion. In this case, the gas flow meter can be set to a temperature lower by about 5 to 8 ° C. than the gas flow control valve. Therefore, it is possible to accurately measure the vaporized gas and control the flow rate thereof with high accuracy. And since the heating apparatus for exclusive use is provided in the material tank, a big thermostat becomes unnecessary.
[0010]
In the second aspect of the present invention, a material tank that contains the liquid material and heats the liquid material to generate a predetermined gas, and a liquid material supply pipe for supplying the liquid material to the material tank, In the liquid material vaporization and supply apparatus comprising a gas outlet pipe for leading out the gas generated in the material tank, the material tank is provided with a heating device for heating it exclusively, and the liquid material supply pipe has the A preheating device for preheating the liquid material supplied to the material tank and a liquid flow rate adjusting device for adjusting the flow rate of the liquid material supplied to the material tank are provided, and a gas flow meter and a gas are provided in the gas outlet pipe provided a flow control valve in a state independent of each other, it is configured to control the temperature individually the gas flow meter and the gas flow control valve, further, the gas flow rate control valve The temperature of the gas tank is higher than the set temperature of the material tank, and the gas flow meter is higher than the set temperature of the material tank and is higher than the gas flow rate control valve. The temperature is controlled so that the temperature is kept low .
[0011]
According to the invention described in claim 2, in addition to the effect of the invention described in claim 1, the following effects can be obtained. That is, according to the second aspect of the present invention, since the liquid material supplied to the material tank is preheated before the supply and the supply amount is limited, vaporization in the material tank is adversely affected. The liquid material can be supplied even during generation of vaporized gas.
[0012]
[0013]
[0014]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the details of the present invention will be described with reference to the drawings. FIG. 1 schematically shows an example of the configuration of a liquid material vaporizing and supplying apparatus according to the present invention. In this figure, reference numeral 1 denotes a material tank which accommodates a liquid material LM and, for example, around the entire periphery excluding its upper surface. A heater 2 as a heating device is provided and is heated and insulated exclusively, and is configured to generate the vaporized gas G by heating the liquid material LM contained therein at a predetermined temperature. Although not shown, the material tank 1 is provided with an appropriate liquid level detection sensor, which detects when the liquid level of the liquid material LM has dropped to a predetermined liquid level and supplies the material. It is configured to output a signal.
[0015]
Reference numeral 3 denotes a liquid material supply pipe for supplying the liquid material LM to the material tank 1, and a preheating device 4 for preheating the liquid material LM supplied to the material tank 1 and adjusting the flow rate of the liquid material LM. The liquid flow rate adjusting device 5 is provided in series in this order, for example, and the liquid material supply pipe 3 on the upstream side of the preheating device 4 is a liquid material supply source (not shown) that stores the liquid material LM via an appropriate pipe. Not connected). And the preheating apparatus 4 consists of heaters, for example, and this is wound around the outer periphery of the liquid material supply pipe 3. The liquid flow rate adjusting device 5 is composed of, for example, a liquid mass flow controller, and is configured to be heated and kept at a predetermined temperature by a heating device 6 such as a heater.
[0016]
Reference numeral 7 denotes a gas outlet pipe for deriving the vaporized gas G generated in the material tank 1. The gas flow meter 8, the gas flow rate control valve 9 and the opening / closing valve 10 are provided in an independent state in this order, for example. The gas outlet pipe 7 on the downstream side of the valve 10 is connected to a use point (not shown) via an appropriate pipe. The gas flow meter 8 is composed of a gas mass flow meter, for example, and is configured to be heated and kept at a predetermined temperature by a heating device 11 such as a heater. The gas flow rate control valve 9 is composed of a gas control valve such as a piezo valve whose opening degree is controlled by a piezo actuator 9a, for example, and is configured to be heated and kept at a predetermined temperature by a heating device 12 such as a heater. ing.
[0017]
Reference numeral 13 denotes a heating device 2 for the material tank 1, a preheating device 4 for the liquid material LM provided in the liquid material supply pipe 3, a heating device 6 for the liquid flow rate adjusting device 5, a heating device 11 for the gas flow meter 8, and a gas flow rate control. Each of the heating devices 2, 4, 6 is a temperature controller that individually controls the temperature of the heating device 12 of the valve 9, based on a command from the personal computer 14 as a control device that controls the entire liquid material vaporization supply device. , 11 and 12 are temperature controlled. The personal computer 14 receives detection outputs from the liquid flow rate adjustment device 5 and the gas flow meter 8 and performs a predetermined calculation based on the detection output to obtain a liquid flow rate and a gas flow rate. Based on the function of outputting a predetermined control signal to the liquid flow rate adjusting device 5 and the gas flow rate control valve 9 based on the detection signal from the liquid level detection sensor provided in the material tank 1 A function to output an opening signal is provided.
[0018]
Next, the operation of the liquid material vaporizing and supplying apparatus having the above configuration will be described. In order to generate the vaporized gas G by heating the liquid material LM in the material tank 1, the desired gas G is generated continuously and stably. In addition, the heating temperature T ° C. of the material tank 1 is set so that vaporization is performed in an optimal state according to the type of the liquid material LM. At this time, the temperature of the preheating device 4 provided in the liquid material supply pipe 3 does not prevent vaporization of the liquid material LM in the material tank 1 even if the liquid material LM preheated thereby is supplied into the material tank 1. Set to about. The liquid mass flow controller 5 as a liquid flow rate adjusting device provided in the liquid material supply pipe 3 is heated and kept at a temperature that does not lower the temperature of the liquid material LM by the heating device 6. On the other hand, the temperature of the gas piezo valve 9 as a gas flow rate control valve provided in the gas outlet pipe 7 is heated and kept at a temperature about 10 ° C. higher than the set temperature T ° C. of the material tank 1 in order to compensate for heat due to adiabatic expansion. The The gas mass flow meter as the gas flow meter 8 provided in the gas outlet pipe 7 is heated and kept at a temperature about 5 to 8 ° C. lower than the set temperature of the gas flow control valve 9.
[0019]
In the liquid material vaporization supply apparatus, the liquid flow rate adjustment apparatus 5 is normally closed. In this state, the material tank 1 containing the liquid material LM is heated by the heating device 2 to increase the internal temperature of the material tank 1 and increase the vapor pressure of the liquid material LM, thereby vaporizing the liquid material LM. A predetermined vaporized gas G is generated. The vaporized gas G is led out to the gas lead-out pipe 7 by obtaining a pressure difference between the material tank 1 and the gas lead-out pipe 7. The gas outlet pipe 7 is provided with a gas flow meter 8 and a gas flow control valve 9 in an independent state. The gas flow control valve 9 is about 10 ° C. higher than the set temperature T ° C. of the material tank 1. Since it is heated and kept at a high temperature, the heat due to adiabatic expansion can be sufficiently supplemented, and the flow rate of the vaporized gas G can be adjusted with high accuracy. Further, since the gas flow meter 8 is heated and kept at a temperature lower by about 5 to 8 ° C. than the gas flow control valve 9, the flow rate of the vaporized gas G can be measured with high accuracy. The vaporized gas G led to 7 flows through the on-off valve 10 at a predetermined flow rate in the direction of the use point.
[0020]
When the liquid material LM in the material tank 1 falls below a certain amount, a predetermined signal is sent from the liquid level detection sensor to the personal computer 14. By this signal input, a predetermined signal is sent from the personal computer 14 to the preheating device 4 and the heating device 6, and these enter a desired heating operation. Then, after a predetermined time has elapsed, the liquid flow rate adjusting device 5 is opened, whereby a new liquid material LM is supplied to the material tank 1. In this case, the liquid material LM to be replenished is heated (preheated) to a predetermined temperature by the preheating device 4 and the supplied amount is limited (adjusted) by the liquid flow rate adjusting device 5. The replenishment of the LM does not prevent the liquid material LM in the material tank 1 from being vaporized. That is, even during replenishment of the liquid material LM, the temperature of the liquid material LM in the material tank 1 does not decrease, but is vaporized by heating, and the generation of the vaporized gas G is maintained.
[0021]
As described above, in the liquid material vaporization supply device having the above-described configuration, the liquid material supply pipe 3 is preheated with the preheating device 4 for preheating the liquid material LM supplied to the material tank 1 and the flow rate of the liquid material LM is adjusted. Since the liquid flow rate adjustment device 5 is provided, the liquid material LM supplied for replenishment when the liquid material LM in the material tank 1 is reduced is preheated before the supply, and the supply amount Therefore, the vaporization in the material tank 1 is not adversely affected, and the liquid material LM can be supplied even during the generation of vaporized gas. Since the gas flow meter 8 and the gas flow control valve 9 provided in the gas outlet pipe 7 for leading the vaporized gas G are independently temperature-controlled so that the respective functions are most exhibited, the vaporized gas G Can be accurately measured and the flow rate can be controlled with high accuracy. Furthermore, since the material tank 1 is heated by the dedicated heating device 2, the temperature can be freely adjusted so that the liquid material LM is vaporized under the best conditions.
[0022]
Further, the heating device 2 is provided in the material tank 1, the preheating device 4 is provided in the liquid material supply pipe 3, the heating device 6 is provided in the liquid flow rate adjusting device 5, the heating device 11 is provided in the gas flow meter 8, and the gas flow rate control is performed. Since the heating device 12 is provided in the valve 9 and these are heated and kept at optimum temperatures, there is no need to provide the thermostatic bath 31 as shown in FIG. 3, and the liquid material is small and compact as a whole. A vaporization supply apparatus can be comprised.
[0023]
The present invention is not limited to the above-described embodiment. For example, as shown in FIG. 2, a gas flow rate control valve 9 that is integrally provided with a pneumatic valve 9B that can be shut off is used. Good.
[0024]
1 and FIG. 2, in the case where a high-temperature mass flow meter is used as the gas flow meter 8 and a large-diameter capillary is used as the sensor portion, the pressure loss in the sensor portion is reduced. This can be reduced, further miniaturization is promoted, and the reliability can be further increased by lowering the temperature.
[0025]
As the liquid flow rate adjusting device 5, a restriction orifice can be used.
[0026]
Further, the arrangement relationship between the preheating device 4 and the liquid flow rate adjusting device 5 in the liquid material supply pipe 3 may be reversed from that in the illustrated example, and further, the gas flow meter 8 and the gas flow rate control valve 9 in the gas outlet pipe 7 may be reversed. The arrangement relationship may be reversed from that in the illustrated example.
[0027]
【The invention's effect】
As described above, according to the liquid material vaporization supply device of the present invention, even when the liquid material is supplied to the material tank, the vaporization of the liquid material in the material tank is not interrupted. Therefore, the liquid material can be continuously and stably vaporized to generate a desired vaporized gas, and the generated vaporized gas can be accurately and stably controlled in flow rate. And since it is not necessary to accommodate a material tank in a thermostat unlike the past, the whole apparatus can be comprised small and compact. That is, according to the present invention, a liquid material vaporizing and supplying apparatus that is small and highly reliable can be obtained.
[Brief description of the drawings]
FIG. 1 is a diagram schematically showing an example of the configuration of a liquid material vaporizing and supplying apparatus according to the present invention.
FIG. 2 is a diagram schematically showing another example of the configuration of the liquid material vaporizing and supplying apparatus.
FIG. 3 is a diagram for explaining a conventional technique.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Material tank, 2 ... Heating apparatus, 3 ... Liquid material supply pipe, 4 ... Preheating apparatus, 5 ... Liquid flow rate adjustment apparatus, 7 ... Gas outlet pipe, 8 ... Gas flow meter, 9 ... Gas flow control valve, LM ... Liquid material, G ... vaporized gas.

Claims (2)

液体材料を収容し、この液体材料を加熱して所定のガスを発生させる材料タンクと、この材料タンクに液体材料を供給するための液体材料供給管と、前記材料タンクにおいて発生したガスを導出するガス導出管を備えてなる液体材料気化供給装置において、前記材料タンクにこれを専用的に加熱する加熱装置を設けるとともに、前記ガス導出管にガス流量計およびガス流量制御弁を互いに独立した状態で設け、前記ガス流量計およびガス流量制御弁を個別に温度制御するように構成され、さらに、前記ガス流量制御弁は、前記材料タンクの設定温度よりも高い温度に加熱保温されるよう温度制御されており、また、前記ガス流量計は、前記材料タンクの設定温度よりも高く、かつ、前記ガス流量制御弁よりも低い温度に加熱保温されるよう温度制御されていることを特徴とする液体材料気化供給装置。A material tank that contains a liquid material and generates a predetermined gas by heating the liquid material, a liquid material supply pipe for supplying the material with the liquid material, and a gas generated in the material tank is led out. In the liquid material vaporizing and supplying apparatus provided with a gas outlet pipe , a heating device for heating the material tank is provided for the material tank, and a gas flow meter and a gas flow control valve are provided in the gas outlet pipe independently of each other. The gas flow meter and the gas flow control valve are individually temperature controlled, and the gas flow control valve is temperature controlled to be heated and maintained at a temperature higher than a set temperature of the material tank. In addition, the gas flow meter is heated and kept at a temperature higher than the set temperature of the material tank and lower than the gas flow control valve. Liquid material vaporizing supply apparatus characterized by being controlled. 液体材料を収容し、この液体材料を加熱して所定のガスを発生させる材料タンクと、この材料タンクに液体材料を供給するための液体材料供給管と、前記材料タンクにおいて発生したガスを導出するガス導出管を備えてなる液体材料気化供給装置において、前記材料タンクにこれを専用的に加熱する加熱装置を設けるとともに、前記液体材料供給管に、前記材料タンクに供給される液体材料を予熱するための予熱装置および材料タンクに供給される液体材料の流量調整を行うための液体流量調整装置を設け、また、前記ガス導出管にガス流量計およびガス流量制御弁を互いに独立した状態で設け、前記ガス流量計およびガス流量制御弁を個別に温度制御するように構成され、さらに、前記ガス流量制御弁は、前記材料タンクの設定温度よりも高い温度に加熱保温されるよう温度制御されており、また、前記ガス流量計は、前記材料タンクの設定温度よりも高く、かつ、前記ガス流量制御弁よりも低い温度に加熱保温されるよう温度制御されていることを特徴とする液体材料気化供給装置。 A material tank that contains a liquid material and generates a predetermined gas by heating the liquid material, a liquid material supply pipe for supplying the material with the liquid material, and a gas generated in the material tank is led out. In the liquid material vaporizing and supplying apparatus provided with a gas lead-out pipe, a heating device for heating the material tank is provided in the material tank, and the liquid material supplied to the material tank is preheated in the liquid material supply pipe. Providing a liquid flow rate adjusting device for adjusting the flow rate of the liquid material supplied to the preheating device and the material tank, and providing the gas outlet pipe with a gas flow meter and a gas flow rate control valve independent from each other, is configured to control the temperature individually the gas flow meter and the gas flow control valve, further, the gas flow control valve, rather than the set temperature of the material tank The temperature of the gas flowmeter is controlled to be higher than the set temperature of the material tank and lower than the temperature of the gas flow rate control valve. liquid material vaporizing supply equipment, characterized in that it is controlled.
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